Azobisisobutyronitrile → 2,6-Dichloro-3-nitrobenzyl Bromide

HRID 342611

반응식

HRID 342611 반응식
[Br:1]C1(Br)NC(=O)NC1=O.[Cl:10][C:11]1[C:16]([N+:17]([O-:19])=[O:18])=[CH:15][CH:14]=[C:13]([Cl:20])[C:12]=1[CH3:21].CC(N=NC(C#N)(C)C)(C#N)C.CC(=O)OCC>ClC1C=CC=CC=1>[Cl:10][C:11]1[C:16]([N+:17]([O-:19])=[O:18])=[CH:15][CH:14]=[C:13]([Cl:20])[C:12]=1[CH2:21][Br:1]

참가 물질

6

반응물 4

HCID 6547AzobisisobutyronitrileHCID 8857Ethyl AcetateHCID 971552,6-Dichloro-3-nitrotolueneHCID 54068228Dibromohydantoin2회

생성물 1

HCID 110115352,6-Dichloro-3-nitrobenzyl Bromide

시약·촉매·용매 1

HCID 7964Chlorobenzene용매

실험 절차

A mixture of dibromohydantoin (70 g, 0.24 mol) and AlBN (5 g) was added in portions at 150° C. to 2,6-dichloro-3-nitrotoluene (100 g, 0.48 mol) in chlorobenzene (400 ml). After 1 h, a mixture of dibromohydantoin (35 g, 0.12 mol) and AIBN (2.5 g) was again added. After a further 1.5 h, the mixture was allowed to cool and EA (500 ml) was added. This mixture was washed once each with saturated Na2SO3, Na2CO3 and NaCl solution, dried (MgSO4) and concentrated, the title compound being obtained as an amorphous powder.

후처리

  1. additionwas again added
  2. waitAfter a further 1.5 h
  3. temperatureto cool
  4. washThis mixture was washed once each with saturated Na2SO3, Na2CO3 and NaCl solution
  5. dry with materialdried (MgSO4)
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-b7a568ba3d00424294d137ce07854653
출처 데이터셋
uspto-grants-1999_01
특허 번호
US05859025

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